fei fib focused ion beam · 2017. 3. 2. · the fib does not know where the sample is in reference...

IF IN DOUBT ASKMick: 255-0650Mick: 255-0650 IF IN DOUBT, ASK

FEI FIB

Focused Ion Beam

Operating Manual

Part 1

IF IN DOUBT ASKMick: 255-0650

Chemical Safety

Users are required to have passed Cornell’s on-line laboratory safety training courses before they can use the FIB.

Do not bring chemicals into the laboratory.

Do not bring hazardous samples or materials into the lab. Contact Mick Thomas or John Grazul with any questions.

This is not a storage facility - do not leave or store samples here. You must take specimens, stubs, and raw material with you when you leave.

Lab-supplied chemicals are limited to a squirt bottle of isopropanol, methanol, and a can of Aero-duster. Wear safety glasses and read the MSDS’s before using them.

A First-Aid kit is provided but this is not a substitute for professional medical help.

Fire escape routes are documented on the following page.

Users failing to follow safety rules will be denied access to the lab.

IF IN DOUBT, ASK

IF ANYTHING UNUSUAL HAPPENS, OR IF THERE ISANYTHING YOU ARE UNSURE ABOUT, STOP ANDCONTACT ME! DO NOT PROCEED OR ATTEMPT TO FIXTHE PROBLEM YOURSELF!

IF IN DOUBT, ASKIF IN DOUBT, ASKMick: 255-0650

1.00


Emergency Shower and Eyewash

Fire Pull Station

In Case of Fire:

Close the door behind youLeave the building

IF IN DOUBT, ASKIF IN DOUBT, ASKIF IN DOUBT, ASKMick: 255-0650

Fire Extinguisher

First Aid Kit

1.00


Gas Safety

Nitrogen gas cylinders are to be changed by CCMR staff members only

Lab Telephone

If you don’t have a cell phone, there is a land-line phone for your use in the corner of the NION room

• Campus Police: 5-1111

• Emergency: 911

• Mick: 255-0650

• John: 255-4130

Illness

If you feel sick, please stay at home. This will require re-scheduling your session, but other people will stay healthy.


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Rules

If ANYTHING does not even SEEMright, leave everything as is and getMick or John

DO NOT attempt to repair ANY part of themicroscope.

DO NOT remove panels, cables, or any part ofthe FIB.

DO NOT add any software or hardware to anycomputer

Flash Drives (Memory Sticks) are forbiddenData MUST be removed by burning a CD

DO NOT bring food or drink into 150.

Wear gloves when handling samples orshuttles.

Individuals failing to follow the rules will bedenied access to the instrument.


2.00


Penalties

Failure to follow these guidelines, unprofessional behavior orcareless use of the equipment will result in loss of permission touse the FIB, in addition to repair charges, if required.

Training requirements

No one is permitted to use the FIB until trained by Mick Thomas.

Room Access

No user is permitted to unlock the door into 150 for the purposeof allowing someone else in to use the FIB.

User Status Signup Room Entry Access

Novice (<2 sessions)

Email ManagerM-F 8am –

5pm

Trained(>2 sessions)

Coral Card SwipeM-F 8am –

5pm

Experienced(>4 sessions)

Coral Card Swipe 24/7

IF IN DOUBT, ASKIF IN DOUBT, ASKMick: 255-0650

2.00


Cancellation

If you sign up and then cannot use your time, cancel your time via Coral or contact Mick at least one weekday before your scheduled time.

Failing to show up

Failure to show up without canceling, unless due to illness or other emergency, can result in use charges

If you fail to show up within 30 minutes of your scheduled starting time the FIB becomes available to other users.

Publication Acknowledgements

When research is published using data from the FIB, the facility and the grant number must be acknowledged, such as:

Data Storage

Data storage and safety is NOT guaranteed!

Users are responsible for their data, and must copy their data to a CD in a timely fashion.

Data will be periodically erased, leaving only one years’ data there.

This work made use of the electron microscopy facilityof the Cornell Center for Materials Research (CCMR)with support from the National Science FoundationMaterials Research Science and Engineering Centers(MRSEC) program (DMR 1120296).


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About this manual (Version 1.0)

This is a limited use manual intended to helpnew users get started on the FEI Focused IonBeam (FIB). It provides information on basicimaging, milling, and TEM sample preparation.It is not intended to be exhaustive, and thereare many principles about focused ion beampractices as well as features of this microscopethat are not covered by this manual. Thismanual will be updated and expanded asneeded.

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Confirm the four circles in the server window turn solid green

If all the circles do not turn solid green then do not proceed – contact Mick

Click on Start

Log on to the xTm Server

Click on Determine

How to start your FIB session

Log into Coral

Log on to Windows on the microscope PC

Click on the FEI System Control icon.

3.00


Understanding the GUI setup:

Activate an image quadrant by clicking in it. The bottom bar will turnblue, indicating that window is now active.

Electron Image Ion image

TV image Status window

Main Toolbar

Controltoolbars

3.00


How to Load a Sample

Click on Navigation Button

Click on Unload in the software

When both lights are green lift the lid

and push Unload/Release

The arm should move away from the

shuttle, allowing you to remove it.

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Note that the two clamping arms must be retracted BEFOREremoving the shuttle

Samples must not exceed the allowable height - check heightusing the height gauge.

They must also fit inside the volume of space as shown at left.

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The shuttle is loaded onto the arm with the three locating balls (rubies) are in the appropriate slots on the arm (inside white circles in picture below).

Gently close the lid and push Clamp/Load.

When loaded the rotation should be -62.4 degrees; if not enter that valueas shown below.

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‐62.4


-10, -10

+10, -10

+10, +10

-10, +10

0, +22

0, 0

How to Find Your Sample in the FIB

Standard stage (at right)

Enter the coordinatesin the boxes for X and Yas shown at right

For TEM stage only:

Front position:X = 0Y = 17

Back position:X = 0Y = -17

3.70


How to Turn On theBeam

Select the upper left handquadrant - this activatesthe electron beam option

Select the voltage and currentfrom the drop -downmenus

Select the Beam Control icon.

Click on Beam On

Un-pause the beam

4.00


?

Electroncolumn

Sample

How to Link Your Sample

The FIB does not know where the sample is in reference to the polepiece(vertical position). The Z value displayed in the Navigation windowwill be wrong. Therefore it is critical to tell the FIB where yoursample is – a process called Linking.

Do not adjust specimen height (Z) until you have Linked at low mag.

Set the magnification to about 50X and focus the beam on the surface ofyour sample

Increase the magnification to about 1000X and refocus

Now STOP – Go no further until you have clicked on the Link icon

4.20


Using the Z control, raise thestage to 9mm, then 7mm,then 5mm, checking aftereach motion that theimage refocuses and theStage motion looksnormal.

If you see a red circle aroundthe Link icon when youreach 5mm then refocusand click on the Link iconagain.

How to Link Your Sample (con’t)

Coarse alignment

4.20



Fine alignment

Find a distinct feature near the area of interest around 1000X magnification.

Tilt the stage by clicking on the drop-down menu and clicking on 15 degrees.

Electroncolumn

15 degrees

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If the feature has moved (down, for example) then move the mouse over the TV image, click on the middle button (the wheel) and a yellow line will appear.

Move the mouse in the direction necessary to move the feature to the middle of the yellow “+” sign on the electron image. As you do this a yellow arrow will appear showing you the direction you are going.

Repeat at 45 degrees (skip 30 degrees), then finally at 52 degrees.

Reset to 0 degrees tilt

Electroncolumn

45 degrees

4.20


How to Select Imaging Conditions

Field-Free: Use for milling and general imaging

Immersion: Use for higher resolution imaging.

EDX: For use while collecting EDX spectra.

How to Select Acquisition Type

Live: Continuous imaging

Average: Uses N number of frames to form an image

Integrate: Takes N frames and then stops

5.00


How to Select Detector Type

ETD: Side mounted detector

TTL: Through the Lens detector

STEM: Transmission detector

CDEM: Channeltron Dynamic Electron Multiplier

CCD: TV image

6.00


7.00 How to Check Beam Alignment

Click on Lens Align to wobble the aperture and reduce wobble, if needed.

Click on Crossover to check the beam centering and improve, if needed.

Correct stigmatism with hardware controls.

You are now ready for electron imaging.


Corrected

Uncorrected

Adjust stigmators

8.00 How to Correct Astigmatism

Adjust the X-stigmator and Y-stigmator so that when you go in and out of focus there is no stretching of the features


Principles of Ion Milling9.00

In the simplest of examples, start with a bulk material with a film on top

Add platinum to protect the sample during milling

Mill away a volume of space to reveal hidden, sub-surface features


9.20 How to set the ion beam conditions

Ion milling can occur at any angle up to about 58 degrees. However it is tyically performed at 52 degrees, when the ion beam is at normal incidence to the sample.

Click in the upper right hand quadrant – the bottom bar should change from gray to blue.

Set the beam current to an appropriate value for your sample, keeping it mind that it is milling your sample all the time you are focusing and stigmating.

Note that there is a very large range of beam currents, with the highest over 10,000 times that of the lowest, so be careful to choose the correct value for your purpose.

The higher the voltage:• The sharper the image• The faster the milling• The more the milling surface will

be amorphized

The higher the current:• The better the S/N• The faster the milling• The bigger the tails on the beam

In the Application drop-down menu select Si


9.20 How to turn on the ion beam

For general milling, make sure the stage is linked and you can tilt to 52 degrees without the feature moving more than 5 um’s

Electroncolumn

52 degrees

If the bar below the Source is gray, click on Wake Up. It will first turn red, then yellow, then green.

When the source is green, click on Beam On.

Remember that imaging with the ion beam is inherently destructive.

Un-pause the beam


How to mill our sample

Select the desired geometric pattern

Draw the desired size or enter it in digitally

Set the depth (Z value)

Click on the Play icon

To stop the milling click on the Stop icon

9.30


How to Deposit Platinum

Choose the Patterning tab

Draw a box where you want to deposit platinum.

Under Gas Injection ‐> Overview right click on “Cold” and a “Heater” optionwill appear.. Left click on “Heater”

Click on white box to the left of Pt Dep to insert needle

9.50

fei fib focused ion beam · 2017. 3. 2. · the fib does not know where the sample is in reference...

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